Diisopropyl Ether → (2Z)-2-[2-(dimethylaminomethylideneamino)-1,3-thiazol-4-yl]-2-methoxyiminoacetyl chloride;hydrochloride

HRID 266245

반응식

HRID 266245 반응식
[Cl-:1].[CH3:2][N:3]([NH+]=C[Cl:7])[CH3:4].[NH2:8][C:9]1[S:10][CH:11]=[C:12](/[C:14](=[N:18]/[O:19][CH3:20])/[C:15]([OH:17])=O)[N:13]=1.[CH:21](OC(C)C)(C)C>O1CCCC1>[ClH:7].[CH3:2][N:3]([CH:4]=[N:8][C:9]1[S:10][CH:11]=[C:12](/[C:14](=[N:18]/[O:19][CH3:20])/[C:15]([Cl:1])=[O:17])[N:13]=1)[CH3:21]

참가 물질

5

반응물 3

HCID 7914Diisopropyl EtherHCID 5486924(alphaZ)-2-Amino-alpha-(methoxyimino)-4-thiazoleacetic acidHCID 86750850Dimethylaminochloromethyleneammonium chloride

생성물 1

HCID 140382097(2Z)-2-[2-(dimethylaminomethylideneamino)-1,3-thiazol-4-yl]-2-methoxyiminoacetyl chloride;hydrochloride수율 96.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-12 °C

실험 절차

Dimethylaminochloromethyleneammonium chloride (1.54 g, 12.0 mmol) was dissolved in 7 ml of tetrahydrofuran, followed by cooling to -12° C. Added to the solution were 1.10 g (5.5 mmol) of (Z)-2-(2-aminothiazol-4-yl)-2-methoxyiminoacetic acid and the resulting mixture was stirred for 40 minutes. Isopropyl ether (16 ml) was added to the reaction mixture, followed by stirring for 40 minutes. Deposited crystals were collected under a nitrogen gas stream, collected by filtration and then dried, whereby 1.65 g of the title compound were obtained (yield: 96.9%).

후처리

  1. additionAdded to the solution
  2. stirringby stirring for 40 minutes
  3. customDeposited crystals were collected under a nitrogen gas stream
  4. filtrationcollected by filtration
  5. customdried

출처 및 근거

ORD 기록
ord-a2d5756d3e9f45d38aee089027d73d8e
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05650518

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